Dimethylformamide → 8-Methoxy-3,4-dihydro-2H-pyrido[2',3':4,5]pyrrolo[2,1-b][1,3]oxazine
反応式
[H-].[Na+].[CH3:3][O:4][C:5]1[CH:6]=[CH:7][C:8]2[N:12]3[CH2:13][C:14]4C([C:11]3=[C:10](C=O)[C:9]=2[N:22]=1)=CC=C[CH:15]=4.CN(C)C=[O:26]>>[CH3:3][O:4][C:5]1[CH:6]=[CH:7][C:8]2[N:12]3[C:11]([O:26][CH2:15][CH2:14][CH2:13]3)=[CH:10][C:9]=2[N:22]=1参加物
4
反応条件
- 温度
- 0 °C
実験手順
Under an inert atmosphere, 160 mg (4 mmol) of sodium hydride (60% in oil) are added slowly at 0° C., to a solution of 380 mg (1.34 mmol) of the compound obtained in Step E in 10 ml of N,N-dimethylformamide. The reaction mixture is stirred at 0° C., for 30 minutes before being hydrolysed with ice and then extracted with ethyl acetate. The organic phase is washed several times with water, dried over magnesium sulphate, concentrated and purified by flash chromatography over silica gel (eluant:ethyl acetate/petroleum ether, 95:5) to yield the title compound in the form of a brown solid.
後処理
- extractionextracted with ethyl acetate
- washThe organic phase is washed several times with water
- dry with materialdried over magnesium sulphate
- concentrationconcentrated
- custompurified by flash chromatography over silica gel (eluant:ethyl acetate/petroleum ether, 95:5)
出典と根拠
- ORDレコード
- ord-211e575ba0fb4516b2c471e468cb0312
- 出典データセット
- uspto-grants-2003_12
- 特許番号
- US06667304B2
反応ノート
読み込み中…